CN109135888A - A kind of complex calcium sulfonate grease and preparation method thereof - Google Patents

A kind of complex calcium sulfonate grease and preparation method thereof Download PDF

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Publication number
CN109135888A
CN109135888A CN201810874411.1A CN201810874411A CN109135888A CN 109135888 A CN109135888 A CN 109135888A CN 201810874411 A CN201810874411 A CN 201810874411A CN 109135888 A CN109135888 A CN 109135888A
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acid
calcium sulfonate
sulfonate grease
calcium
complex calcium
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李嘉
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QINGDAO GUANGLIANDA PRECISION MACHINERY Co Ltd
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QINGDAO GUANGLIANDA PRECISION MACHINERY Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/04Mixtures of base-materials and additives
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06Metal compounds
    • C10M2201/062Oxides; Hydroxides; Carbonates or bicarbonates
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/085Phosphorus oxides, acids or salts
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/087Boron oxides, acids or salts
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02Hydroxy compounds
    • C10M2207/021Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/04Ethers; Acetals; Ortho-esters; Ortho-carbonates
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/121Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
    • C10M2207/122Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms monocarboxylic
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/121Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
    • C10M2207/123Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/126Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/128Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/14Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/141Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings monocarboxylic
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/06Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • C10M2215/064Di- and triaryl amines
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/044Sulfonic acids, Derivatives thereof, e.g. neutral salts
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/08Resistance to extreme temperature
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10Semi-solids; greasy

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  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

The invention belongs to technical field of lubricating grease, a kind of complex calcium sulfonate grease and preparation method thereof is disclosed.In terms of mass fraction, the lubricating grease includes following components: base oil, 30~70 parts, 30~70 parts of calcium sulfonate with high base number, 1~10 part of composite transformation agent, 1~4 part of low molecular acid, 1 1~10 part of dihydroxystearic acids, 1~5 part of calcium hydroxide, 0.5~5 part of structural improvement agent, 1~10 part of nanometer additive, 0.1~1 part of antioxidant.The high-performance grease of calcium sulfonic acid excellent combination property, water resistant performance of flushing, high temperatures and mechanical stability are substantially better than similar product.

Description

A kind of complex calcium sulfonate grease and preparation method thereof
Technical field
The invention belongs to technical field of lubricating grease, and in particular to a kind of complex calcium sulfonate grease and preparation method thereof.
Background technique
Grease of calcium sulfonic acid is a kind of new multi-purpose lubricating grease, have excellent high temperature resistance, extreme pressure and antiwear behavior, Mechanical stability energy and rustless property.Have the more patents about grease of calcium sulfonic acid both at home and abroad, CN103103012A is introduced A kind of stearic acid modified grease of calcium sulfonic acid, improves the variation of appearance after lubricating grease is contacted with water.CN102417855B A kind of calcium sulfonate tetra-polyurea lubricating grease is described, the advantage and disadvantage of grease of calcium sulfonic acid and polyurea grease has been neutralized, has provided A kind of water repelling property and the more excellent product of bearing life.But water repelling property evaluation method involved in above scheme compares It is relatively mild, lubricating grease cannot be embodied completely in the application operating condition of harsh environment.
Summary of the invention
In view of this, the present invention provides a kind of novel complex calcium sulfonate grease, which is meeting GB/ Under the premise of T33585-2017 performance requirement, there is more excellent comprehensive performance, especially water resistant performance of flushing.Therefore more Add suitable for the harsh application for being easy to contact water, such as metallurgy industry conticaster, hot rolling mill, coastal waters pier facilities, boat Transport the lubrication and protection of equipment etc..
Technical scheme is as follows:
The present invention provides a kind of complex calcium sulfonate grease, comprises the following components in parts by weight:
Base oil: 30~70 parts;
Calcium sulfonate with high base number: 30~70 parts;
Composite transformation agent: 1~10 part;
Low molecular acid A:0.5~2 part;
Low molecular acid B:0.5~4 part;
Ten dihydroxystearic acids: 1~10 part;
Calcium hydroxide: 1~5 part;
Structural improvement agent: 0.5~5 part;
Nanometer additive: 1~10 part;
Antioxidant: 0.1~1 part.
Preferably, the base oil is refined paraffin wax base oil, in naphthene base crude oil, synthesis hydrocarbon, synthesizing ester oil, alkylnaphthalene One or more of mixtures.
Preferably, the calcium sulfonate with high base number is the synthesis type sulfoacid calcium of 300~400mgKOH/g of total base number, mahogany acid Or mixtures thereof calcium.
Preferably, the composite transformation agent is two kinds in low mass molecule alcohol, low molecule ether, organic acid and low molecule inorganic acid Or a variety of mixtures.
Preferably, the low molecular acid A is one of formic acid, acetic acid and oxalic acid.
Preferably, the low molecular acid B is one of boric acid, phosphoric acid and acetic acid.
Preferably, the structural improvement agent is ethylene propylene copolymer, polyisobutene, styrene isoprene copolymers, line One of type polymethacrylates, star-like polymethacrylates, modified ethylene propylene copolymer are a variety of.
Preferably, the nanometer additive is in nanometer calcium carbonate, nano-titanium oxide, nano zine oxide and nano aluminium oxide It is one or more.
Preferably, the antioxidant is in di-iso-octyldiphenylamine, dinonyldiphenylamine and di-tert-butyl p-cresol It is a kind of.
The present invention also provides the preparation methods of above-mentioned complex calcium sulfonate grease, comprising the following steps: first will be high-alkali Value sulfoacid calcium, part basis oil are mixed with composite transformation agent, obtain mixture;Mixture is warming up to 50-70 DEG C, is added low point Sub- acid A, then 70~90 DEG C are warming up to, keep the temperature 30~60 minutes;Calcium hydroxide emulsion, the aqueous solution of low molecular acid B is added in sequence And ten dihydroxystearic acids, it is reacted 30~120 minutes at 90~100 DEG C;170~180 DEG C are warming up to, remaining base oil is added; Structural improvement agent, nanometer additive and antioxidant dispersion are added when temperature is lower than 90 DEG C, obtains the Composite calcium-sulfonate-batetrapolyurea Lubricating grease.
Compared with the prior art, the advantages of the present invention are as follows:
Complex calcium sulfonate grease of the invention has more under the premise of meeting GB/T33585-2017 performance requirement Add excellent comprehensive performance, especially water resistant performance of flushing, high temperatures and mechanical stability.Therefore it is more applicable for the easy of harshness In contact water application, as metallurgy industry conticaster, hot rolling mill, coastal waters pier facilities, equipment for shipping, engineering machinery, The lubrication and protection of heavy-load automobile etc..
Specific embodiment
The present invention provides a kind of complex calcium sulfonate grease, has excellent comprehensive performance, especially water resistant erosion Can, it is applicable to various industrial applications.Lubricating grease of the invention comprises the following components in parts by weight:
Base oil: 30~70 parts;
Calcium sulfonate with high base number: 30~70 parts;
Composite transformation agent: 1~10 part;
Low molecular acid A:0.5~2 part;
Low molecular acid B:0.5~4 part;
Ten dihydroxystearic acids: 1~10 part;
Calcium hydroxide: 1~5 part;
Structural improvement agent: 0.5~5 part;
Nanometer additive: 1~10 part;
Antioxidant: 0.1~1 part.
In complex calcium sulfonate grease of the invention, based on parts by weight, base oil accounts for 30~70 parts, preferably 34~ 60 parts, more preferably 40~50 parts.Base oil of the invention refers to grease base plinth material or basestocks concoction, by single Manufacturer produces (independent of feed source or the place of manufacturer) according to same size;Meet the specification of same manufacturer; And by being uniquely formulated, product ID or the two identified.In the present invention, base oil can be paraffine base crude oil, cycloalkanes One or more of base oil, synthesis hydrocarbon, synthesizing ester oil, alkylnaphthalene mixture, such as 500SN, 150BS, PAO100.If When two or more mixtures, the present invention does not limit the mixed proportion of base oil each in mixture, arbitrary proportion.This Invention does not have particular/special requirement to the source of base oil and type, can be it is any be currently known or find later for just it is any It is applied to prepare grease base plinth oil with all such, is such as applied to engine oil, marine cylinder oil, functional liquid is for example hydraulic Oil, gear oil, transmission oil etc..Those skilled in the art can make proper amount of other additions disclosed by the invention by routine techniques Agent and base oil prepare lubricating grease of the invention jointly.
In complex calcium sulfonate grease of the invention, based on parts by weight, calcium sulfonate with high base number accounts for 30~70 parts, preferably It is 35~60 parts, more preferably 40~50 parts.In the present invention, the calcium sulfonate with high base number base number is 300-400mgKOH/g newton Or mixtures thereof body high base number calcium mahogany sulfonate or calcium alkylbenzenesulfonate.
In complex calcium sulfonate grease of the invention, based on parts by weight, composite transformation agent accounts for 1~10 part, preferably 3 ~6 parts, more preferably 4~5.5 parts.In the present invention, the composite transformation agent is low mass molecule alcohol, low molecule ether, organic acid and low Two or more of mixtures in molecule inorganic acid.In the present invention, the low mass molecule alcohol, low molecule ether, organic acid and low molecule Inorganic acid is in this field to compound well known to the skilled person, the low mass molecule alcohol, such as methanol, ethyl alcohol, different Propyl alcohol, n-butanol etc.;The low molecule ether, such as ethylene glycol monomethyl ether, ethylene glycol ethyl ether;The organic acid for example benzoic acid, oleic acid, Benzene sulfonic acid etc.;Described inorganic acid such as boric acid, phosphoric acid etc..The type and ratio that the present invention mixes composite transformation agent do not have special limit System, those skilled in the art can according to need to be selected in above compound.
In complex calcium sulfonate grease of the invention, based on parts by weight, low molecular acid A accounts for 0.5~2 part, preferably 1 ~1.5 parts.In the present invention, one of the preferred formic acid of the low molecular acid, acetic acid and oxalic acid, more preferably acetic acid.Low molecule Sour A have stronger acid reactivity, can rapidly and raw material in calcium carbonate reaction, release carbon dioxide, facilitate calcium carbonate The change of crystal form.
In complex calcium sulfonate grease of the invention, based on parts by weight, low molecular acid B accounts for 0.5~4 part, preferably 1 ~3 parts, more preferably 1.5~2.5 parts.The low molecular acid B is preferably one of boric acid, phosphoric acid and acetic acid, more preferably Boric acid or phosphoric acid.Low molecular acid B is for improving lubricating grease extreme pressure and antiwear behavior.
In complex calcium sulfonate grease of the invention, based on parts by weight, containing 0.5~5 part of structural improvement agent, preferably It is 1~4 part, more preferably 2~3 parts.Structural improvement agent of the present invention is mainly used for improving product stability energy, adhesion property And water repelling property.The structural improvement agent is high molecular polymer, preferably ethylene propylene copolymer, polyisobutene, styrene One of isoprene copolymers, line style polymethacrylates, star-like polymethacrylates, modified ethylene propylene copolymer Or it is a variety of, more preferably styrene isoprene copolymers, star-like polymethacrylates, in modified ethylene propylene copolymer It is one or more.Modified ethylene propylene copolymer of the present invention is preferably the 2002D of Lubrizol company.
It is based on parts by weight, excellent containing 0.1~1 part of antioxidant in complex calcium sulfonate grease of the invention It is selected as 0.3~0.8 part, more preferably 0.5~0.6 part.In the present invention, the antioxidant is preferably diisooctyl hexichol One of amine, dinonyldiphenylamine and di-tert-butyl p-cresol.
In complex calcium sulfonate grease of the invention, based on parts by weight, containing 1~10 part of nanometer additive, preferably It is 1.5~5 parts, more preferably 2~4 parts.In the present invention, the nanometer additive be preferably nanometer calcium carbonate, nano-titanium oxide, One of nano zine oxide and nano aluminium oxide are a variety of.The nanometer additive is for improving lubricating grease extreme pressure anti-wear Energy.
The invention also includes the preparation methods of above-mentioned complex calcium sulfonate grease, include the following steps:
Calcium sulfonate with high base number, part basis oil are mixed with composite transformation agent first, obtain mixture;Mixture is warming up to Low molecular acid A is added in 50~70 DEG C, preferably 55~65 DEG C;Temperature is warming up to 70~90 DEG C again, keeps the temperature 30~60 minutes, 75~85 DEG C are preferably warming up to, keeps the temperature 40~50 minutes;Sequence be added calcium hydroxide emulsion, the aqueous solution of low molecular acid B and Ten dihydroxystearic acids are reacted 30~120 minutes at 90~100 DEG C, are preferably reacted 40~100 minutes at 92~97 DEG C;It rises Temperature is to 170~180 DEG C, the remaining base oil of preferably 173~178 DEG C additions;When temperature be lower than 90 DEG C when be added structural improvement agent, Nanometer additive and antioxidant dispersion, obtain the complex calcium sulfonate grease.
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that Described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the implementation in the present invention Example, every other embodiment obtained by those of ordinary skill in the art without making creative efforts belong to The scope of protection of the invention.
The product of following producer is selected in following embodiments of the invention, but is not limitation of the present invention.
150BS base oil: 40 DEG C of kinematic viscosity 100cSt, producer such as Exxon Mobil Corporation, Sinopec, Chinese stone Oil.
Calcium sulfonate with high base number: total base number is the calcium alkylbenzenesulfonate of 300~400mgKOH/g, and total base number is 400mgKOH/g's Calcium mahogany sulfonate, producer such as Lubrizol Corporation.
Amine type antioxidant: di-iso-octyldiphenylamine, dinonyldiphenylamine, producer such as Lubrizol Corporation.
Structural improvement agent: Lubrizol 2002D, producer such as Lubrizol Corporation.
Nanometer additive: nanometer calcium carbonate, nano-titanium oxide, nano zine oxide, the expensive Xingda in producer such as Beijing.
Embodiment 1:
606g150BS base oil, 1212g calcium alkylbenzenesulfonate (total base number 400mgKOH/g), 76g benzoic acid and 80g ethyl alcohol Mixing.50 DEG C are heated to, is added 30g acetic acid (being pre-dispersed in 2 times of water), is warming up to 70 DEG C, keeps the temperature 30 minutes.36g is added Calcium hydroxide (is pre-dispersed in 2 times of water).It is added 57g boric acid (being pre-dispersed in 2 times of boiling water), ten dihydroxy of 78g is added Stearic acid.It is reacted 120 minutes at 90 DEG C.174 DEG C are warming up to, 606g 150BS base oil is added.It is lower than 90 DEG C to temperature of charge When be added 150g nanometer calcium carbonate, 60g Lubrizol2002D, 15g di-iso-octyldiphenylamine antioxidant.It is dispersed after degassing i.e. Obtain finished product.
Finished product detection data are shown in Table 1.
Embodiment 2:
By 606g150BS base oil, 1320g calcium alkylbenzenesulfonate (total base number 300mgKOH/g), 60g oleic acid and 100g second two The mixing of alcohol methyl ether.60 DEG C are heated to, is added 30g oxalic acid (being pre-dispersed in 2 times of water), is warming up to 80 DEG C, keeps the temperature 45 minutes.Add Enter 36g calcium hydroxide (being pre-dispersed in 2 times of water), be added 57g phosphoric acid (being pre-dispersed in 2 times of boiling water), 78g 12 is added Hydroxy stearic acid.It is reacted 80 minutes at 96 DEG C.180 DEG C are warming up to, 606g 150BS base oil is added.It is lower than 90 to temperature of charge DEG C when be added 60g nano-titanium oxide, 150g Lubrizol2002D, 5g dinonyldiphenylamine antioxidant.After being dispersed degassing It gets product.
Finished product detection data are shown in Table 1.
Embodiment 3:
631.5g150BS base oil, 1365g calcium mahogany sulfonate (total base number 400mgKOH/g), 100g boric acid and 62g methanol Mixing.70 DEG C are heated to, is added 30g acetic acid (being pre-dispersed in 2 times of water), is warming up to 90 DEG C, keeps the temperature 60 minutes.36g is added Calcium hydroxide (is pre-dispersed in 2 times of water), is added 57g boric acid (being pre-dispersed in 2 times of boiling water), and ten dihydroxy of 78g is added Stearic acid.It is reacted 60 minutes at 100 DEG C.170 DEG C are warming up to, 631.5g 150BS base oil is added.It is lower than 90 to temperature of charge DEG C when be added 100g nano zine oxide, 30g Lubrizol2002D, 9g di-iso-octyldiphenylamine antioxidant.It is dispersed degassing After get product.
Finished product detection data are shown in Table 1.
Examples 1 to 3 high base number composite calcium sulfonate base grease performance is measured, and is washed away using lubricating grease water resistant Test ASTM D4049 is measured, and the results are shown in Table 1.
The comparison of the PERFORMANCE OF GREASES of the lubricating grease of the present invention of table 1 and the prior art
Wherein, comparative example is complex calcium sulfonate grease conventional in the prior art.
As can be seen from Table 1, complex calcium sulfonate grease of the invention can satisfy the performance of GB/T33585-2017 It is required that.Horizontal compared with the existing technology simultaneously, i.e. comparative example in table 1 has better water resistant performance of flushing and high-temperature oxidation resistant Performance.Therefore it is more applicable for the harsh application for being easy to contact water, such as metallurgy industry conticaster, hot rolling mill, coastal waters Pier facilities, the lubrication and protection of equipment for shipping etc..
Present invention employs lubricating grease water resistant washout test ASTM D4049 to the just evaluation of lubricating grease water repelling property, should Test it is harsher, can more embody the difference of different composite grease of calcium sulfonic acid water repelling property, while having excellent high temperatures And mechanical stability.
Above-described specific embodiment has carried out further the purpose of the present invention, technical scheme and beneficial effects It is described in detail, it should be understood that being not intended to limit the present invention the foregoing is merely a specific embodiment of the invention Protection scope, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should all include Within protection scope of the present invention.

Claims (10)

1. a kind of complex calcium sulfonate grease, which is characterized in that comprise the following components in parts by weight:
Base oil: 30~70 parts;
Calcium sulfonate with high base number: 30~70 parts;
Composite transformation agent: 1~10 part;
Low molecular acid A:0.5~2 part;
Low molecular acid B:0.5~4 part;
Ten dihydroxystearic acids: 1~10 part;
Calcium hydroxide: 1~5 part;
Structural improvement agent: 0.5~5 part;
Nanometer additive: 1~10 part;
Antioxidant: 0.1~1 part.
2. complex calcium sulfonate grease according to claim 1, which is characterized in that the base oil be paraffine base crude oil, One or more of naphthene base crude oil, synthesis hydrocarbon, synthesizing ester oil, alkylnaphthalene mixture.
3. complex calcium sulfonate grease according to claim 1, which is characterized in that the sulfoacid calcium is total base number 300 Or mixtures thereof the synthesis type sulfoacid calcium of~400mgKOH/g, calcium mahogany sulfonate.
4. complex calcium sulfonate grease according to claim 1, which is characterized in that the composite transformation agent is low molecule Two or more mixtures in alcohol, low molecule ether, organic acid and low molecule inorganic acid.
5. complex calcium sulfonate grease according to claim 1, which is characterized in that the low molecular acid A is formic acid, second One of acid and oxalic acid.
6. complex calcium sulfonate grease according to claim 1, which is characterized in that the low molecular acid B is boric acid, phosphorus One of acid and acetic acid.
7. complex calcium sulfonate grease according to claim 1, which is characterized in that the structural improvement agent is ethylene propylene Alkene copolymer, styrene isoprene copolymers, line style polymethacrylates, star-like polymethacrylates, changes polyisobutene One of sex ethylene propylene copolymer is a variety of.
8. complex calcium sulfonate grease according to claim 1, which is characterized in that the nanometer additive is nano-sized carbon One of sour calcium, nano-titanium oxide, nano zine oxide and nano aluminium oxide are a variety of.
9. complex calcium sulfonate grease according to claim 1, which is characterized in that the antioxidant is diisooctyl One of diphenylamines, dinonyldiphenylamine and di-tert-butyl p-cresol.
10. a kind of preparation method of complex calcium sulfonate grease described in claim 1~9 any one, it is characterised in that: packet It includes following steps: calcium sulfonate with high base number, part basis oil being mixed with composite transformation agent, obtain mixture;Mixture is heated up To 50~70 DEG C, low molecular acid A is added, then be warming up to 70~90 DEG C, keeps the temperature 30~60 minutes;Calcium hydroxide cream is added in sequence Liquid, the aqueous solution of low molecular acid B and ten dihydroxystearic acids react 30~120 minutes at 90~100 DEG C;It is warming up to 170~ 180 DEG C, remaining base oil is added;Structural improvement agent, nanometer additive and antioxidant point are added when temperature is lower than 90 DEG C It dissipates, obtains the complex calcium sulfonate grease.
CN201810874411.1A 2018-08-03 2018-08-03 A kind of complex calcium sulfonate grease and preparation method thereof Pending CN109135888A (en)

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CN109762632A (en) * 2019-01-15 2019-05-17 广西碳酸钙产业化工程院有限公司 Calcium carbonate high-performance complex calcium sulfonate grease and preparation method thereof
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